Combustion Nitrogen Analyzers

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Feb 22, 2014 (3 years and 5 months ago)

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Combustion Nitrogen Analyzers

elementar Americas, Inc.

SERA
-
IEG Annual Meeting

June 21, 2009







1

Combustion

Nitrogen Analyzers

Agenda

elementar Americas Inc.

history and current organization

elementar product line

applications overview

Analyzer technology and operation

Chemistry / Process flow / Mechanical design

Selecting an instrument

design considerations

choices
-

Rapid N cube / vario MACRO cube / vario MAX



2

3

elementar history

Technology Development

1868
-

high temperature techniques developed in Hanau, Germany

1878
-

Dennstedt Patent

1925
-

Nobel prize for CHN analysis

1990
-

first Macro scale elemental analyzer

1999
-

first MAX analyzer

2006
-

first cube platform analyzer introduced


Organization

1868
-

Heraeus

1993
-

management buyout forms elementar GmbH

1999
-

elementar Americas Inc formed

2008
-

Isoprime Ltd acquired
(Isotope Ratio Mass Spectrometers)


4

elementar Organization

Manufacturing, R&D and applications labs

elementar Analysensysteme GmbH

CHNS/O Elemental Analyzers

Located in Hanau, Germany (30 minutes from Frankfurt Airport)

Isoprime Ltd

Wholly owned subsidiary

Isotope Ratio Mass Spectrometers

Located near Manchester, U.K


Sales, service, applications, and supplies

elementar Americas, Inc.

Responsible for sales and service in USA, Canada, Mexico and Central America

based in Mt. Laurel, NJ (30 minutes from Philadelphia)

Service from NJ, IN, CO, Toronto


5

elementar

Elemental Analyzer Product Line

Micro scale CHNS/O

vario MICRO cube

vario EL cube

Macro scale CHNS/O

vario MACRO cube

vario MAX

rapid N cube & rapid CS cube

TOC

liquiTOC

vario TOC cube

6

vario MAX
CN

Macro N/CN Elemental Analyzers

rapid N
cube

vario
MACRO CN
cube

Elemental Analyzer

Technology and Operation

Core Operations

Combustion

Gas separation

Gas detection

Chemistry

Process Flow Diagram

Other operations

Sample preparation

Autosampler and sample feeding

Software


7

8

Elemental Analyzer

Core Operations

Combustion

Sample combusts in furnace at
950 deg C to 1200 deg C

Sample drops into crucible or is
lowered into center of
combustion tube

Jet injection of oxygen via lance
right over/at sample

Creates turbulent flow around
sample

like blowing on a fire

Three tube low voltage furnace
with 10 year warranty

9

Elemental Analyzer

Core Operations

Gas Separation

Helium or CO
2

carrier gas
pushes combustion gases
through analyzer.

C, H and S combustion gases
are trapped in separate
columns, then sequentially
released (aka “purge and trap”).

N
2

gas is not trapped. It flows
straight thru columns.


Gas Detection

TCD


Thermal Conductivity Detector

Utilizes a Wheatstone bridge circuit to
compare relative thermal conductivity
differences between the carrier gas and
analyte gas

Critical system component

Elementar own design

Larger dynamic range

Very special thermistors which are not
harmed by high oxygen content.

Allows for suspension of carrier gas flow
without any harm, even at operation
temperature.


Elemental Analyzer

Core Operations

11

Elemental Analyzer

Chemistry

Combustion

R
-
N + O
2

----
> N
2

+ NO
x

+ O
2

+ CO + CO
2

+ CH
4

+ X
-

+

SOx + H
2
O


Post Combustion

CO + CH
4

---
CuO & Pt

--
> CO
2

+ H
2
O


Reduction

NO
x
+O
2

+SO
2
--
tungsten
--
> N
2
+WO
3
+CO (trace)

CO + CuO
--------
> CO
2


12

Elemental Analyzer

More Chemistry

Removal of other gases

X
-


via reaction with silver wool

H
2
O

via condensation, membrane dryer and Sicapent

trace
S0
2

via reaction with tungsten



Nitrogen

detected by TCD


Carbon Dioxide

rapid N


“fades” into carrier gas

vario MAX and vario MACRO


separated on purge and trap
column, then released and detected by TCD.

N
2

CO
2


CO + CH
4

---
CuO

& Pt
--
> CO
2

+
H
2
O

R
-
N + O2

----
>

CO + CO
2

+ CH
4

+ N2 + NO
x

+ SO
x
+ H
2
O + X
-

+ O2


sample

CO

CH
4

X

X

X

NOx

H
2
O

X

N
2

SO
2

X

X

X
-

X

CO
2

O
2

NO
x

+ CH
4
+O
2

+SO
2
--
tungsten
--
> N
2
+WO
3
+CO
(trace)


WO
3

CO
2

CO
2

N= 2.00%

C= 3.00%

Oxidation

Post Oxidation

Reduction

Process Flow Diagram and Chemistry


Gripper Arm lowers crucible
containing sample into combustion
tube


Oxygen is injected over sample


Sample combusts


Combustion gasses are produced


We are interested in N
2

and CO
2
.


Other gases must be converted
or removed.




Methane and carbon dioxide are
oxidized in post combustion tube.


Carbon dioxide flows through
instrument and is trapped in
column

Halogens are removed by reaction
with silver wool in post
combustion tube.



Water is removed by a three stage
dryer:


condensation


membrane dryer


Sicapent

Reduction Tube


Excess oxygen reacts with
Tungsten.


SO2 is adsorbed by tungsten.


O
2

Reduction Tube:


Oxides of nitrogen reduce to
nitrogen gas.


Nitrogen flows to TCD.


Computer integrates peak and
calculates N
2

percent.


CO2 column is heated.


CO2 flows to TCD.


Computer integrates peak and
calculates CO
2

percent.



Ash

Ash


Gripper arm removes crucible
with ash from combustion tube.


Crucible deposited in recepticle
for re
-
use



Process Flow Diagram Comparison

14

Replace robotic
arm with Carousel
and ball valve

vario MACRO cube CN

Replace robotic
arm with Carousel
and ball valve

Rapid N cube

CO2

Remove CO2
adsorber

Add CF Hybrid

Elemental Analyzer

Technology and Operation

Core Operations

Combustion

Gas separation

Gas detection

Chemistry

Process Flow Diagram

Other operations

Sample preparation

Autosampler and sample feeding

Software

15

Sample Preparation

rapid N cube and vario MACRO cub
e

16

60 position open carousel


-

add samples at any time during run


-

optional 80 or 120 position carousel

Variety of foils/capsules

Sample Pressing Tool

17


rapid N cube and vario MACRO cube have
slightly different designs.



Both designs provide:


inherent blank
-
free system


reliable function


keeps air out of the system


very long lasting operation


easy maintenance

Ball Valve Sample Feed

rapid N cube and vario MACRO cub
e

18

rapid N Sample Introduction

Ball valve with nickle flap flange


Straight
-
through Ball Valve
actuates.



Sample falls to top of nickel
flap flange.



Nickel flap flange actuates
magnetically.


vario MACRO cube

patented zero
-
blank ball
valve


Position 1; Sample falls into ball valve
cavity.



Position 2; Ball valve cavity purged
with helium.



Position 3; Ball valve opens to
combustion tube.

Position #1

Position #2

Position #3

20

vario Max

Sample preparation

21

vario MAX

sample feeding

22

vario Max

Sample Feeding

Robotic “gripper arm”

Lifts reusable crucible from
carousel.

Lowers crucible into the
combustion tube (~1000
o

C)

Lifts to removes crucible and
ash

Deposits the ash & crucible in
catch bin

23

Analyzer Software


intuitive
interface


easy editing


view graph
during
analysis


great export
functionality


21CFR
part11/LIMS
/GLP
conformity

Elemental Analyzer

Technology and Operation

Core Operations

Combustion

Gas separation

Gas detection

Chemistry

Process Flow Diagram

Other operations

Sample preparation

Autosampler and sample feeding

Software

24



1000



300

Sample



Size

200

(mg Organic



Content)

50



10

















C

S

N

CN

CNS

CHNS

CHN

O

Cl

Operating Mode



25

Macro sample N/CN Analyzer Selection


maximum capacity (organic) and
capability



26

Vario MAX

Best choice for CN or N samples that are
non
-
homogeneous, very low in concentration, wet , high ash
or difficult to handle.

Vario MACRO cube

Optimum economics for larger CN samples with easier
handling characteristics (dry, semi
-
homogeneous).

Capital cost lower than MAX

CF Hybrid technology optimizes consumables cost

Rapid N cube

Optimum economics for larger N samples with easier
handling characteristics.

Capital cost lower than MACRO

CO
2

carrier gas reduces gas cost

Macro sample N/CN Analyzer Selection

recommendations

vario MACRO cube

Elementar
´
s answer to YOUR
analytical needs

The new cost
-
effective macro analyzer
family for



N/CN

for protein, plant material or
soil analysis



CNS


CHNS

for plant and soil,
environmental or oil samples




CHN

for the analysis of coal,
biomass or combustible solid waste

Options:



„Standard options:“

-

Capsule press for liquids

-

Pressing tool


IR Detectors for special applications:

-

low level sulfur analysis

-

low level oxygen analysis

-

chlorine analysis



VLS, vario liquid sampler



Continuous flow Hybrid (CN only)

Options:

Automatic liquid injector for the „cube“ family



liquid sample feeder for 60
samples, plus flushing and
waste positions




easy setup, replaces standard
ball valve and carousel




can be used on:



vario EL cube



vario MICRO cube



vario MACRO cube




Launched in 2008, first
installations successful

CF
-
Hybrid technique for CN
mode

The newly developed hybrid technology serves for longer lifetime of
consumables.

Only a fraction (approx 50%, adjustable) of the combustion gas is
lead through the reduction tube in continuous flow mode, saving
valuable reduction metal and expansion of uninterrupted operation
time.



Features:



Easy to install and remove (1
-
2 minutes!), so the user can
choose between highest sensitivity or highest throughput.



Active flow control.



Ideal for high
-
throughput laboratories with similar sample
matrix.

Elementar thanks you for
your attention !

For further information please contact
us under:


Web Page: www.CHNOS.com


e
-
mail: info@elementar
-
inc.com